🔥🔥 Don’t Miss Out on Our End of Autumn Sale. If you have any questions, feel free to click the bottom right corner to contact our customer service..

Concat us[email protected]
Shopping Cart

No products in the cart.

🔍
BS EN 17683:2023

BS EN 17683:2023

$198.66

Animal feeding stuffs. Methods of sampling and analysis. Determination of pyrrolizidine alkaloids in animal feeding stuff by LC-MS/MS

Published By Publication Date Number of Pages
BSI 2023 70
PDF Format Searchable Printable Preview Now
Guaranteed Safe Checkout
Category:

If you have any questions, feel free to reach out to our online customer service team by clicking on the bottom right corner. We’re here to assist you 24/7.
Email:[email protected]

This document describes a method for the quantitative determination of pyrrolizidine alkaloids (PA) in complete and supplementary feed and in forages by liquid chromatography tandem mass spectrometry (LC-MS/MS) after solid phase extraction (SPE) clean-up. The method has been successfully validated in a collaborative trial for the matrices complete feed for horses, supplementary feed for horses, supplementary feed for rodents, hay, alfalfa and grass silage. Validation was carried out for the PA and concentrations ranges listed in Table 1. It was demonstrated that the PA isomeric pairs senecivernine and senecionine as well as senecivernine-N-oxide and senecionine-N-oxide cannot be determined individually due to insufficient chromatographic separation. However, the sums of the individual PA of the isomeric pairs were quantified with sufficient reproducibility. Co-elution of other PA-isomers not included in the scope of the method shall be taken into account. A list of potentially co-eluting isomers is presented in Annex E. Although the calibration range of the method protocol is specified from 10 μg/kg to 300 μg/kg, the results of the collaborative study showed, that the dilution of sample extracts with blank sample extracts enables for the quantitation of concentrations exceeding the calibration range. Satisfactory reproducibility was achieved when quantifying up to 1428 μg/kg for individual PA and up to 887 μg/kg for the sum of isomeric pairs. NOTE 1 A second method was part of the method validation collaborative main trial. For this method PA-N-Oxides are reduced by adding zinc powder to the extract of the feed material. The following steps correspond to the first and main method. Quantitative results for each PA except the otonecine type PA senkirkine represent the sum of the free PA base and its corresponding N-oxide. NOTE 2 Due to insufficient numbers of data for some analyte-matrix combinations statistical evaluation was not valid for standardization. Received data indicated the methods applicability in experienced laboratories with appropriate quality assurance measures. Therefore, the method description is included as an informative annex (Annex D).

PDF Catalog

PDF Pages PDF Title
2 undefined
8 1 Scope
9 2 Normative references
3 Terms and definitions
4 Principle
12 5 Apparatus
13 6 Procedure
16 7 HPLC-MS/MS analysis
17 8 Results
19 9 Precision
20 10 Test report
21 Annex A (informative)Precision data
A.1 General
54 Annex B (informative)Example of LC-MS/MS conditions
B.1 General
B.2 Chromatographic conditions
55 B.3 Mass spectrometric conditions
57 Annex C (informative)Example LC-MS/MS chromatogram of a pyrrolizidine alkaloid mixture
58 Annex D (informative)Method protocol for the determination of pyrrolizidine alkaloids in animal feeding stuff by LC-MS/MS after reduction of N-oxides using metallic zinc
D.1 General
D.2 Introduction
D.3 Principle
D.3.1 General
59 D.3.2 Reagents
D.3.3 Analytical Standards
D.3.4 Chemicals
D.3.4.1 General
D.3.4.2 zinc powder, analytical grade
D.3.5 Solutions
D.3.5.1 General
D.3.5.2 Free PA-bases working solution, 1 µg/ml
D.3.5.3 PA-N-oxides working solution, 1µg/ml
D.3.6 Apparatus
D.3.7 Procedure
D.3.7.1 General
60 D.3.7.2 Sample preparation
D.3.7.3 Extraction
D.3.7.4 SPE procedure
D.3.7.5 Reconstitution of the sample
D.3.7.6 Quality control samples
61 D.3.7.7 Calibration by means of matrix matched standards (MMS)
D.3.8 HPLC-MS/MS analysis
D.3.9 Results
D.3.9.1 Peak identification
D.3.9.2 Calibration function
D.3.9.3 Quantification
D.3.9.4 Reporting of results
D.3.9.5 Quality control – performance criteria
62 D.4 Results
D.5 Method performance data
D.5.1 Method performance data obtained during single laboratory validation
63 D.5.2 Method performance data obtained during collaborative trial
67 D.6 Report
68 Annex E (informative)List of potentially co-eluting pyrrolizidine alkaloid (PA) isomers

Related products

BS EN 17683:2023
$198.66